Reaktion #467930

Reaktionsgleichung

6-chloro-N-methyl-4-o-tolyl-nicotinamide

1-methylpiperazine

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product

Ausbeute 83.7%

N-Methyl-6-(4-methyl-piperazin-1-yl)-4-o-tolyl-nicotinamide

Ausbeute 83.7%

Lösungsmittel

NaOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted
2. 2
   SonstigeThe aqueous phase was separated
3. 3
   Extraktionextracted twice with THF
4. 4
   Waschenthe organic phases were washed twice with brine
5. 5
   TrocknenThe combined organic phases were dried over Na2SO4
6. 6
   Sonstigethe solvent was removed under reduced pressure
7. 7
   Sonstigethe residue purified by chromatography over silica gel (CH2Cl2:MeOH=99:1)

Vorschrift

A solution of 3.2 g (12.2 mmol) 6-chloro-N-methyl-4-o-tolyl-nicotinamide in 6.7 ml (60.3 mmol)1-methylpiperazine was stirred at 100° C. for 2.5 h. The reaction mixture was cooled to r.t., treated with 10 ml 0.1N NaOH and extracted. The aqueous phase was separated and extracted twice with THF and the organic phases were washed twice with brine. The combined organic phases were dried over Na2SO4, the solvent was removed under reduced pressure and the residue purified by chromatography over silica gel (CH2Cl2:MeOH=99:1) to yield 3.3 g (83.7%) product as a beige foam.

Quelle